CN103258954B - gas sensor based on flexible substrate and preparation method thereof - Google Patents
gas sensor based on flexible substrate and preparation method thereof Download PDFInfo
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- CN103258954B CN103258954B CN201210036092.XA CN201210036092A CN103258954B CN 103258954 B CN103258954 B CN 103258954B CN 201210036092 A CN201210036092 A CN 201210036092A CN 103258954 B CN103258954 B CN 103258954B
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Abstract
The invention discloses a kind of gas sensor based on flexible substrate and preparation method thereof, this gas sensor is followed successively by from the bottom up: substrate, bottom electrode, sensitive membrane and upper electrode; Wherein, this sensitive membrane is between bottom electrode and upper electrode, and its section is exposed so that gas with sensitive membrane effect, gives full play of the sensitivity characteristic of sensitive membrane at this section. Gas sensor based on flexible substrate provided by the invention and preparation method thereof, compared to traditional plane sensitive membrane, there is three-dimensional sensitive character, it is prone to contacting of tested gas and all sensitive membrane, play the interlaminar action of sensitive membrane greatly, it is achieved function under room temperature or high temperature, special gas is sensitive.
Description
Technical field
The present invention relates to gas sensor technology field, particularly relate to a kind of gas sensor based on flexible substrate and preparation method thereof.
Background technology
At present, along with the raising of the development of social technology and people's living standard, in field of food safety, pharmaceutical sanitary field for sensor light, small-sized, flexible detection become more and more urgent. Gas sensor based on rigid substrate is highly developed, but, its application scenarios is subject to the restriction of substrate itself, it is impossible to meet market demands, so, flexible substrate has good development potentiality.
Air-sensitive film comparatively popular at present generally or is apply after mix homogeneously, or is be processed to form two membranes at twice, without being further processed. So, when analyzing sensitivity characteristic, just much pind down. Such as, for sensitive membrane, in a lot of situations, it is impossible to form comparatively single nonwoven fabric from filaments, even if defining single nonwoven fabric from filaments, gas also is difficult to arrive between each layer nonwoven fabric from filaments, and this cannot play effect produced by layer and interlayer contact. When mixture, generally it is difficult to produce specific periodic structure: superlattices, and superlattices itself have a lot of unique character, in enough periodic regimes, it is possible to produce conduction band character. So, overcoming problem in above-mentioned two situations, the raising for air-sensitive performance can produce active influence.
Summary of the invention
(1) to solve the technical problem that
In view of this, a kind of gas sensor based on flexible substrate of offer and preparation method thereof is provided.
(2) technical scheme
For reaching above-mentioned purpose, the invention provides a kind of gas sensor based on flexible substrate, this gas sensor is followed successively by from the bottom up: substrate, bottom electrode, sensitive membrane and upper electrode; Wherein, this sensitive membrane is between bottom electrode and upper electrode, and its section is exposed so that gas with sensitive membrane effect, gives full play of the sensitivity characteristic of sensitive membrane at this section.
In such scheme, this sensitive membrane adopts three layers sensitive membrane or multi-layer sensitive film, and all adopts sandwich. for three layers sensitive membrane, adopting ABC structure, this ABC structure is followed successively by the first metal-oxide (A), organic high molecular polymer (B) and the second metal-oxide (C) from bottom to top, for multi-layer sensitive film, adopt ABAB ... structure or ABCABC ... structure, this ABAB ... structure is followed successively by the first metal-oxide (A) from bottom to top, organic high molecular polymer (B), first metal-oxide (A), organic high molecular polymer (B) ..., this ABCABC ... structure is followed successively by the first metal-oxide (A) from bottom to top, organic high molecular polymer (B), second metal-oxide (C), first metal-oxide (A), organic high molecular polymer (B), second metal-oxide (C) .... described first metal-oxide (A) and the second metal-oxide (C) all play the effect of auxiliary sensitive, strengthen with the sensitivity characteristic according to himself or weaken the described organic high molecular polymer (B) susceptiveness to certain gas, enabling the concentration of this sensor selective enumeration method specific gas. for multi-layer sensitive film, adopt ABAB ... structure or ABCABC ... structure, it is possible to form superlattice structure.
In such scheme, the pattern of this sensitive membrane sandwich is circular, oval, square, rectangle or irregular figure. In this sensitive membrane, organic high molecular polymer (B) adopts PPy or PANi, and the first metal-oxide (A) and the second metal-oxide (C) adopt MoO3��SnO2, ZnO, NiO or TiO2In the combination of any one or any two kinds.
In such scheme, this bottom electrode and upper electrode play the effect of conduction, described sensitive membrane are connected with peripheral circuit, and bottom electrode and upper electrode adopt metal electrode or have the non-metal electrode MWCNTS composition of strong electric conductivity.
For reaching above-mentioned purpose, the preparation method that present invention also offers a kind of gas sensor based on flexible substrate, the method includes: deposit layer of metal electrode, spin coating one layer photoetching glue on metal electrode on substrate; This photoresist it is exposed and develops, forming photoetching agent pattern; By spin coating, it is deposited with or is deposited on the substrate forming photoetching agent pattern and be sequentially depositing three layers or multi-layer sensitive film; And in sensitive membrane, deposit electrode, through once peeling off molding.
In such scheme, in the described step depositing layer of metal electrode on substrate, selecting PI thin film or PET film as substrate, metal electrode selects metallic copper, is made by E-beam depositing technics. Described substrate thickness is 75 microns to 125 microns, and the deposition thickness of metal electrode is 30nm-100nm.
12, the preparation method of the gas sensor based on flexible substrate according to claim 10, it is characterized in that, described on metal electrode in the step of spin coating one layer photoetching glue, negative glue 5214 chosen by photoresist, sol evenning machine setting speed 1000 and 1 minute time, metal electrode forms the negative gel coating of thickness 3.5 microns.
In such scheme, described photoresist be exposed and develop, formed in the step of photoetching agent pattern, it is substrate is placed on the hot plate of 80 DEG C, dries 4 points 30 seconds, then carry out graph exposure, time of exposure 4 seconds, again substrate is placed on the hot plate of 120 DEG C, dries 2 minutes, expose 20 seconds when maskless version afterwards; Double exposure power is held at 60W; Develop subsequently; After exposure imaging, mask graph region is covered by a layer photoetching glue, and non-graphic region is then dissolved, and forms photoetching agent pattern.
In such scheme, described by spin coating, be deposited with or be deposited on formed photoetching agent pattern substrate on be sequentially depositing in the step of three layers or multi-layer sensitive film, spin coating proceeding is with the process applying photoresist, evaporation process adopts E-Beam technique evaporation oxidation thing material or adopts the mode of thermal evaporation to evaporate organic polymer material, and depositing technics is for utilizing LPCVD technique one layer of oxide of deposit; Choosing of sensitive membrane, for organic high molecular polymer sensitive membrane, its thickness is 0.2 micron-10 microns; For metal oxide party, its thickness is 0.1 micron-2 microns.
In such scheme, described in sensitive membrane, deposit electrode, in the step once peeling off molding, stripping is shaped to conventional stripping process, successively substrate is respectively put in isopropanol, acetone and ethanol and soaks each 10 minutes to remove the covering on photoresist and photoresist, clean about 10 minutes with deionized water again, to remove the organic solvent of residual in above step.
(3) beneficial effect
From technique scheme it can be seen that the method have the advantages that
1, gas sensor based on flexible substrate provided by the invention and preparation method thereof, compared to traditional plane sensitive membrane, there is three-dimensional sensitive character, it is prone to contacting of tested gas and all sensitive membrane, play the interlaminar action of sensitive membrane greatly, it is achieved function under room temperature or high temperature, special gas is sensitive.
2, gas sensor based on flexible substrate provided by the invention and preparation method thereof, multilayer film put in order and the number etc. of film can arbitrarily convert.
Accompanying drawing explanation
Fig. 1 is the profile of the gas sensor based on flexible substrate according to the embodiment of the present invention;
Fig. 2 is the top view of the gas sensor based on flexible substrate according to the embodiment of the present invention;
Fig. 3 is the manufacture method flow chart of the gas sensor based on flexible substrate according to the embodiment of the present invention.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Gas sensor based on flexible substrate provided by the invention and preparation method thereof, three layers (or multilamellar) sensitive membrane is adopted to be contacted with ambient atmos by tangent plane, contact surface is designed to network structure, be conducive to increasing contact area, and be conducive to playing the interaction of different sensitive interlayer, it is easy to accomplish feature specific to superlattices.
As illustrated in fig. 1 and 2, gas sensor based on flexible substrate provided by the invention, with flexible insulating material (including PI, PET, special paper material) for substrate, with the electric parameter such as electric capacity or resistance for signal output, with laminated construction for reaction interface structure, it is achieved the test to special gas. This gas sensor is followed successively by from the bottom up: substrate, bottom electrode, three layers or multi-layer sensitive film, upper electrode. Wherein, this three layers or multi-layer sensitive film are between bottom electrode and upper electrode, and the section of this three layers or multi-layer sensitive film comes out so that gas at section with sensitive membrane effect, can give full play of the sensitivity characteristic of sandwich. Bottom electrode and upper electrode play the effect of conduction, sensitive membrane are connected with peripheral circuit. Bottom electrode and upper electrode adopt metal electrode or have non-metal electrode (such as the MWCNTS) composition of strong electric conductivity.
Sensitive membrane adopts sandwich, is followed successively by the first metal-oxide (A), organic high molecular polymer (B), the second metal-oxide (C) from bottom to top, as shown in Figure 1. For multiple structure (more than three layers), adopt ABAB ... or ABCABC ... etc. form. Metal-oxide (A) and metal-oxide (C) all play the effect of auxiliary sensitive, can strengthen or weaken the organic high molecular polymer (B) susceptiveness to certain gas according to they self sensitivity characteristic, make this sensor can the concentration of selective enumeration method specific gas. According to ABAB ... or ABCABC ... form, it is possible to form superlattice structure, increase electrical conductivity, reduce resistance, it is simple to test.
The various patterns such as the pattern of laminated construction can be circular, oval, square, rectangle, irregular figure. The size Control of whole device is within the scope of 50 microns �� 50 microns to 1cm �� 1cm. Single contact pattern area can be minimum to 0.5 micron2Magnitude. The general thickness of sensitive layer is minimum for several nanometers, each layer according to concrete sensitive material, thickness is minimum for several nanometers.
Choosing of sensitive membrane: in sensitive membrane, organic high molecular polymer (B) can adopt PPy or PANi, the first metal-oxide (A) and the second metal-oxide (C) can adopt MoO3��SnO2, ZnO, NiO or TiO2In the combination of any one or any two kinds. Selective coating is carried out according to surveyed gas. Coated form includes the methods such as drop coating, dip-coating, thermal evaporation, printing, E-Beam, CVD, PVD.
Based on the gas sensor shown in Fig. 1 and Fig. 2, Fig. 3 illustrates the manufacture method flow chart of the gas sensor based on flexible substrate according to the embodiment of the present invention, the method is first to deposit layer of metal electrode on substrate, the photoresist that spin coating is one layer relatively thick on metal electrode, this photoresist is exposed and develops, the photoetching agent pattern of formation shadow region shape as shown in Figure 2; The means such as spin coating, evaporation or deposit that then pass through are sequentially depositing three layers or multi-layer sensitive film on the substrate forming photoetching agent pattern, then deposit electrode in sensitive membrane, through once peeling off molding. Specifically comprise the following steps that
Step 1: selecting PI thin film or PET film as substrate, substrate thickness is 75 microns to 125 microns.
Step 2: deposit layer of metal electrode on substrate; Metal electrode selects the metal simple-substance higher with electric conductivity such as copper, is made by E-beam depositing technics, between the optional scope 30nm-100nm of deposition thickness.
Step 3: the photoresist that spin coating is a layer relatively thick on metal electrode, is exposed this photoresist and develops;
Photoresist chooses negative glue 5214, sol evenning machine setting speed 1000 and 1 minute time, forms the negative gel coating of thickness 3.5 microns on metal electrode. Exposure process: be placed on by substrate on the hot plate of 80 DEG C, dries 4 points 30 seconds, then carries out graph exposure, time of exposure 4 seconds, then is placed on by substrate on the hot plate of 120 DEG C, dries 2 minutes, exposes 20 seconds when maskless version afterwards. Double exposure power is held at 60W. Develop subsequently.
Step 4: after exposure imaging, mask graph region is covered by a layer photoetching glue, and non-graphic region is then dissolved, the photoetching agent pattern of formation shadow region shape as shown in Figure 2.
Step 5: be sequentially depositing three layers or multi-layer sensitive film on the substrate forming photoetching agent pattern by means such as spin coating, evaporation or deposits, concrete technology is as follows: spin coating proceeding is similar to the process of coating photoresist, evaporation process adopts E-Beam technique evaporation oxidation thing material or adopts the mode of thermal evaporation to evaporate organic polymer material, and depositing technics is for utilizing LPCVD technique one layer of oxide of deposit. Choosing of sensitive membrane, for organic high molecular polymer sensitive membrane, its thickness is 0.2 micron-10 microns, metal oxide party, and its thickness is 0.1 micron-2 microns, if both mixture, its thickness range 0.2 micron-10 microns.
Step 6: electrode on depositing in sensitive membrane, through once peeling off molding.
The technique depositing electrode in sensitive membrane is identical with bottom electrode technique, and upper thickness of electrode is identical with bottom electrode.
Stripping is shaped to conventional stripping process, successively substrate is respectively put in isopropanol, acetone and ethanol and soaks each 10 minutes to remove the covering on photoresist and photoresist, clean about 10 minutes with deionized water again, to remove the organic solvent of residual in above step. Obtain the covering part outside shadow region in Fig. 1.
Particular embodiments described above; the purpose of the present invention, technical scheme and beneficial effect have been further described; it is it should be understood that; the foregoing is only specific embodiments of the invention; it is not limited to the present invention; all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (12)
1. the gas sensor based on flexible substrate, it is characterised in that this gas sensor is followed successively by from the bottom up: substrate, bottom electrode, sensitive membrane and upper electrode; Wherein, this sensitive membrane is between bottom electrode and upper electrode, and its section is exposed so that gas at this section with sensitive membrane effect;
Wherein, this sensitive membrane adopts three layers sensitive membrane or multi-layer sensitive film, and all adopts sandwich;
For three layers sensitive membrane, adopting ABC structure, this ABC structure is followed successively by the first metal-oxide A, organic high molecular polymer B and the second metal-oxide C from bottom to top;
For multi-layer sensitive film, adopt ABAB ... structure or ABCABC ... structure, this ABAB ... structure is followed successively by the first metal-oxide A, organic high molecular polymer B, the first metal-oxide A, organic high molecular polymer B from bottom to top ..., this ABCABC ... structure is followed successively by the first metal-oxide A, organic high molecular polymer B, the second metal-oxide C, the first metal-oxide A, organic high molecular polymer B, the second metal-oxide C from bottom to top ....
2. the gas sensor based on flexible substrate according to claim 1, it is characterized in that, described first metal-oxide A and the second metal-oxide C all plays the effect of auxiliary sensitive, strengthen with the sensitivity characteristic according to himself or weaken the described organic high molecular polymer B susceptiveness to certain gas, enabling the concentration of this gas sensor selective enumeration method specific gas.
3. the gas sensor based on flexible substrate according to claim 1, it is characterised in that for multi-layer sensitive film, adopts ABAB ... structure or ABCABC ... structure, it is possible to form superlattice structure.
4. the gas sensor based on flexible substrate according to claim 1, it is characterised in that the pattern of this sandwich is circular, oval, rectangle or irregular figure.
5. the gas sensor based on flexible substrate according to claim 1, it is characterised in that in sensitive membrane, organic high molecular polymer B adopts PPy or PANi, the first metal-oxide A and the second metal-oxide C to adopt MoO3��SnO2, ZnO, NiO or TiO2In the combination of any one or any two kinds.
6. the gas sensor based on flexible substrate according to claim 1, it is characterized in that, this bottom electrode and upper electrode play the effect of conduction, sensitive membrane are connected with peripheral circuit, and bottom electrode and upper electrode adopt metal electrode or non-metal electrode MWCNTS to constitute.
7. the method preparing the gas sensor based on flexible substrate according to any one of claim 1 to 6, the method includes:
Substrate deposits layer of metal electrode, spin coating one layer photoetching glue on metal electrode;
This photoresist it is exposed and develops, forming photoetching agent pattern;
By spin coating or be deposited on formed photoetching agent pattern substrate on be sequentially depositing three layers or multi-layer sensitive film; And
Electrode on depositing in sensitive membrane, through once peeling off molding;
Wherein, described by spin coating or be deposited on formed photoetching agent pattern substrate on be sequentially depositing in the step of three layers or multi-layer sensitive film,
Spin coating proceeding is with the process applying photoresist, and depositing technics adopts E-Beam technique evaporation oxidation thing material, or adopts the mode of thermal evaporation to evaporate organic polymer material, or utilizes LPCVD technique one layer of oxide of deposit;
Choosing of sensitive membrane, for organic high molecular polymer, its thickness is 0.2 micron-10 microns; For metal-oxide, its thickness is 0.1 micron-2 microns.
8. the preparation method of the gas sensor based on flexible substrate according to claim 7, it is characterized in that, in the described step depositing layer of metal electrode on substrate, select PI thin film or PET film as substrate, metal electrode selects metallic copper, is made by E-beam depositing technics.
9. the preparation method of the gas sensor based on flexible substrate according to claim 8, it is characterised in that described substrate thickness is 75 microns to 125 microns, and the deposition thickness of metal electrode is 30nm-100nm.
10. the preparation method of the gas sensor based on flexible substrate according to claim 8, it is characterized in that, described on metal electrode in the step of spin coating one layer photoetching glue, negative glue 5214 chosen by photoresist, sol evenning machine setting speed 1000 and 1 minute time, metal electrode forms the negative gel coating of thickness 3.5 microns.
11. the preparation method of the gas sensor based on flexible substrate according to claim 7, it is characterized in that, described this photoresist it be exposed and develop, being formed in the step of photoetching agent pattern, being place the substrate on the hot plate of 80 DEG C, dry 4 points 30 seconds, then carry out graph exposure, time of exposure 4 seconds, then place the substrate on the hot plate of 120 DEG C, dry 2 minutes, expose 20 seconds when maskless version afterwards; Double exposure power is held at 60W; Develop subsequently; After exposure imaging, mask graph region is covered by a layer photoetching glue, and non-graphic region is then dissolved, and forms photoetching agent pattern.
12. the preparation method of the gas sensor based on flexible substrate according to claim 7, it is characterised in that described deposit electrode in sensitive membrane, in the step once peeling off molding,
Stripping is shaped to conventional stripping process, successively substrate is respectively put in isopropanol, acetone and ethanol and soaks each 10 minutes to remove the covering on photoresist and photoresist, clean 10 minutes with deionized water again, to remove the organic solvent of residual in above step.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015085537A1 (en) * | 2013-12-12 | 2015-06-18 | 中国科学院微电子研究所 | Sensor module based on flexible substrate |
| CN105319241A (en) * | 2014-07-04 | 2016-02-10 | 中国科学院苏州纳米技术与纳米仿生研究所 | Flexible gas-sensitive sensor and making method thereof |
| CN104568002B (en) * | 2014-12-26 | 2017-05-03 | 昆山工研院新型平板显示技术中心有限公司 | Environmental detection device |
| CN106167287A (en) * | 2016-07-25 | 2016-11-30 | 杨林 | A kind of gas separation equipment for sewage treatment area |
| KR102000592B1 (en) * | 2017-07-04 | 2019-07-16 | 주식회사 엔디디 | Bio-sensing device and methods of fabricating the same |
| CN107870225B (en) * | 2017-11-06 | 2020-05-19 | 浙江科丰传感器股份有限公司 | Flexible three-dimensional packaging gas sensor |
| CN108226098B (en) * | 2017-12-20 | 2020-12-22 | 中国科学院微电子研究所 | Fano resonance optical hydrogen sensor and preparation method and application system thereof |
| CN110987260B (en) * | 2018-03-20 | 2021-04-30 | 武汉铂纳智感科技有限公司 | Flexible electronic skin capable of sensing pressure and air sensitivity simultaneously and preparation method thereof |
| CN108982600B (en) * | 2018-05-30 | 2021-07-09 | 杨丽娜 | Flexible gas sensor based on gallium oxide/zinc gallate heterojunction nano array and preparation method thereof |
| CN108535337B (en) * | 2018-05-30 | 2021-04-20 | 杨丽娜 | Flexible gas sensor based on tin oxide/gallium oxide heterojunction nano array and preparation method thereof |
| CN111243966B (en) * | 2020-01-14 | 2021-11-05 | 联合微电子中心有限责任公司 | Flexible sensor manufacturing process and flexible sensor |
| CN116577382B (en) * | 2023-07-12 | 2023-09-29 | 长春理工大学 | Gas sensor based on light excitation, preparation method and application thereof |
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